1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → tert-butyl 1-((4-(5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)-1-piperidinyl)carbonyl)pentylcarbamate

To a solution of 2-((tert-butoxycarbonyl)amino)hexanoic acid (0.46 g) obtained in Example 80a), HOBt (0.46 g) and WSC (0.58 g) in acetonitrile (20 ml) was added a solution of 5-methyl-2-(4-piperidinyl)-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride (0.6 g), DBU (0.6 ml) and triethylamine (0.61 ml) in acetonitrile (20 ml), and mixed for 15 hours. The solvent was distilled off under reduced pressure, and the residue was dissolved in dichloromethane. The dichloromethane solution was washed with an aqueous sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified with basic silica gel column (ethyl acetate/methanol=10/1) to obtain the title compound as colorless powder (0.7 g, 75%).

1. additionmixed for 15 hours
2. distillationThe solvent was distilled off under reduced pressure
3. dissolutionthe residue was dissolved in dichloromethane
4. washThe dichloromethane solution was washed with an aqueous sodium hydrogen carbonate solution
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified with basic silica gel column (ethyl acetate/methanol=10/1)

ORDレコード

ord-6d4679d0c3cf47f1a8f37e2da8b73118

出典データセット

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07820673B2